Textile fabric and method of preparation thereof



Patented Nov. 10, 1942 UNITED STATEVS'YIPATENTI OFF ICE TEXTILE FABRICAND METHOD or mnmm'rron 'rnsanor William W. Trowell, Greenville, 8.0.,assignor to Hercules Powder Company, Wilmington, Del., a corporation ofDelaware Nc Drawing.

Application July 22, 1939,

Serial No. 285,965

7 Claims.

' This invention relates to a method of simul-:

taneously dyeing and finishing a textile fabric,

and more particularly to an improved method of producing a dyed textilefabric having a permanent finish.

Oneobject of this invention is to provide a method for producing apermanently sized, dyed textile fabric having a superior dye fastness towashing fluids and having a finish which is resistant to laundering. Afurther object of this invention is to providea method of simultaneouslydyeing and permantstuif, removing the'excess emulsion from the fabric,evaporating the water and volatile solvent from the. impregnated fabric,and pressing the fabric at an elevated temperature.

In carrying out the method in accordance with this invention, a textilefabric is impregnated with an aqueous emulsion of a solution ofwater-insoluble ethyl cellulose in a volatile, substantiallywater-immiscible solvent, the said aqueous emulsion containing in thewater phase a direct, watersoluble dyestufi. A plasticizer for the ethylcellulose which is substantially inert to the action of aqueous alkalineWashing solution and also a synthetic resin of suitable type may beincluded in the emulsion if desired.

, In following my method, the excess emulsion may be convenientlyremoved from the fabric by passing the cloth between padded squeezerolls. The fabric is then preferably dried at an elevated temperature toremove the water and volatile solvent from the impregnated fabric andthen pressed or ironed preferably at a temperature within the range ofabout 180 F. to about 400 F., and more preferably within the range ofabout 240 F. to about 280 F., the actual temperature used beingdependent upon the type of fabric employed and the particularcomposition deposited on the fabric. complished by passing the treatedfabric over a series of heated rolls or by drying the fabric in a Theironing process may be acblast of heated air and subsequently passing itbetween heated pressure rolls.

The amount of emulsion remaining in the fabric after removal of theexcess by passing between the padded squeeze rolls will determine to alarge extent the final stillness, hand and body of the finished dyedfabric. By impregnating the fabrics with emulsions containing differentconcentrations of ethyl cellulose with or without the plasticizers andsynthetic resins it is possible to vary the amount of solids depositedin thefabric and thereby to vary-the hand and body of the finishedfabric as desired. In any event, the

" amount of emulsionremaining in the fabric after the excess emulsionhas been removed will be such that the amount of dry, film-formingcomposition remaining in thefabric will, at the end of my procedure, beinsuflicient to fill the interstices between threads or to form acontinuous coating over the surface of the fabric, but will besufiicient to provide the finished fabric herein described.

In practicing my invention, I apply my ethyl cellulose emulsionscontaining a direct water-soluble dye in the water phase so as to leavein the finished dyed fabric an amount of the thermoplastic substance inthe drystate not over about 40% of the weight of the untreated fabric,and preferably not over about 20% of the weight of the untreated fabric.The amount of dry thermoplastic substance retained in the fabric iscontrolled depending on whether a soft, flexible, permanent finish onthe one hand or a stiff, starched-like finish on the other hand, or anyfinish intermediate thereto'is desired.

The ethyl cellulose used in the aqueous emulsions of this invention willbe sufficiently etherified to be insoluble in water and inorganicsolvents and will be recognized as water-insoluble ethyl cellulose. Itmay have, for example, an ethoxy content in the range of about 43% toabout 51%, and preferably from about 44% to about 48%.

The viscosity characteristics of the ethyl cellulose used will dependupon the properties desired in the ultimate composition.

The aqueous emulsion of water-insoluble ethyl cellulose, used inaccordance with my invention 'they contributeto the fullness and body ofthe finished fabric more than the liquid plasticizers. Suitableplasticizers are hydrogenated methyl abietate; hydrogenated ethylabietate; triphenyl phosphate; tricresyl phosphate; tributyl phosphate;methyl phthalyl methyl glycollate; ethyl dilute the concentratedemulsion.

phthalyl ethyl glycollate; di-(para-tertiary butyl phenyl),mono-(5-tertiary butyl-2 xenyl) phosphate, etc.

The aqueous emulsion may also contain a suitable synthetic resin. Resinswhich I have found to be suitable in my invention are thermoplastic,alkali-resistant synthetic resins compatible with ethyl cellulose. Thus,I have found that I may use rosin-modified alkyd resins, such as rosinmodified or hydrogenated rosin modified terpenemaleic anhydride resins,rosin modified maleate resins; drying oil modified terpene-maleicanhydride resins; polymerized hydrocarbon resins, such as polymerizednaphthalene, polymerized coumarone-indene or hydrogenated forms,vthereof; 100% phenolic resins; polyhydric alcohol esters of hydrogenatedrosin, as well as resins of other types which are of a thermoplasticcharacter, are alkali-resistant and are compatible with ethyl cellulose.Where optimum results are desirable, I prefer to employ resins fallingwithin the above classification which are light in color and which havea relatively low acid number.

The aqueous ethyl cellulose emulsions used in accordance with thisinvention will preferably be prepared by emulsifying in water awater-immiscible solution of water-insoluble ethyl cellulose or ofwater-insoluble ethyl cellulose mixed with either a plasticizer or asynthetic resin, or both, in a suitable common solvent therefor,preferably a mixed solvent comprising light aromatic and petroleumhydrocarbons and butanol. The emulsions will be of the oil-in-watertype. Suitable emulsifying agents are, for example, the alkali metalsalts of the higher aliphatic half ester sulfates, as sodium laurylsulfate, sodium stearyl sulfate, etc.; sulfonated oils, as sulfonatedcastor fil, sulfonated olive oil, etc.; soaps, as sodium te,-potassiumoleate; sodium oleate, etc.; metal salts of alkyl naphthalene sulfonicstear alka acids, as sodium butyl naphthalene sulfonate My improvedprocess of simultaneously finishing and dyeing textile fabrics isapplicable to any of the textile materials such as for example, organdy,lace, broadcloth, cotton, wool, rayon, etc. Naturally, due to thedifferent qualities of fabric to be treated, their weight, their degreeof absorbency, etc., it is impossible to define the amount ofimpregnating composition required to provide either a soft, flexiblefinish or a stiff, starched-like finish. Generally speaking, however, amaximum of about 40% by weight of solid thermoplastic substance in thefabric, based on the weight of the untreated fabric, is contem-Pontamine Fast Red 8BL l 278 Pontamine Fast Green GL None PontamineYellow CH 365 Pontamine Sky Blue FF 518 Pontamine Fast Brown RKL NonePontamine Fast Orange Pr 56 Pontamine Black E 581 Pontamine Blue BBNConc 406 Pontamine Brown BT Conc 561 Pontamine Brown RMR 420 PontamineFast Black FF 539 Pontamine Fast Blue RRL 319 Pontamine Fast Brown BRLlPr 41 Pontamine Fast Orange ERL Pr 56 Pontamine Fast Orange MRL 621Pontamine Fast Orange S 326 Pontamine Fast Red F 419 Pontamine FastScarlet 4BA 326 Pontamine Fast Yellow 4GL Conc Pr 43 Pontamine YellowNNL 814 plated. For most purposes, not over about 20% by weight iscontemplated.

The concentration of the solid ingredients of the emulsions used in myinvention may be varied over wide ranges merely by diluting concentratedExample I H The following solutions were prepared:

Parts by weight (a) Ethyl cellulose 32 Xylnl 122 Hi flash naphtha 26Butanol 20 Total 200 (b) Potassium oleate 1.5 Water 98.5

Total Two hundred parts by weight of solution (a) were pro-mixed with100 parts by weight of solution (b) by pouring solution (alginto thewater phase while agitating the latter and emulsified together bypassing the pre-mixed emulsion twice through a Manton-Gaulin two-stagehomogenizer usingabout 2,000 pounds pressure on the first stage andabout 2,500 pounds pressure on the second stage so that a particle sizeof about 5 microns to about 50 microns was obtained. Five hundred partsby weight of the emulsion were then diluted with 1,000 parts by weightof water containing 3.75 parts by weight of Pontamine fast red 8BL. Thedyestuff was ture before addition to the concentrated emulf-g;

sion. The diluted emulsion containing the dyestuff so obtained was thenused to simultaneously impregnate and dye 2.85 yard sheeting. The excessemulsion was squeezed from the fabric and the fabric dried over dry cansat a temperature of about 275 F. The dyed and finished fabric obtainedpossessed a full-bodied, semi-stiff finish and had a stiffness of 33 mg.as measured on a Gurley stiffness tester. The fabric possessed improveddye strength and more level dyeing over that obtained without the use ofthe ethyl cellulose emulsion.

Example 11 Solutions (a) and (b) were emulsified as in Example I. Theconcentrated emulsion wasdiluted with a dye solution containingPontamine fast red 831. as in Example I, and the diluted emulsioncontaining the dyestufi used to simultaneously dye and finish 2.85 yardsheeting as in Example I. The resulting fabric had a full, stifi finish,the stiffness being 96.3 mg. as measured on the Gurley stiffness tester.The dyed fabric possessed greater depth of shade and more level dyeingthan obtainable without the ethyl cellulose emulsion. The dyedfabricretained its color and stiffness after laundering.

' Example VI Five hundred parts by weight of the concentrated emulsionused in Example III were di luted with 1,000 parts by weight of watercontaining 3.75 parts by weight of Pontamine fast green GL (DuPont). Themixture contained 0.25% dye. The diluted emulsion was used tosimultaneously impregnate and dye 2.85 yard sheeting by the proceduredescribed in Example Example I. The resulting fabric had a stillness Iof 39.6 mg. The dyed fabric obtained was resistant to washing andretained its stiffness after Solutions (a) and (b) were emulsified as inExample I. The simultaneous dyeing and finishing procedure of Example Iwas repeated. The fabric obtained possessed a stiff hand having astiffness of 90.2 mg. The dyed strength was greater than obtainedwithout the ethyl cellulose emulsion and the fabricrretained its dye andfinish on laundering.

Example IV 0 Five hundred parts by weight of the concentrated ethylcellulose emulsion used in Example III were'diluted with 1,000 parts byweight of water containing 3.75 parts by weight of Pontamine yellow CH.The diluted emulsion contained 0.25% dye. It was used to impregnate 2.85yard sheeting by the procedure described in Example I. The resultingfabric was full-bodied and still, having a stiffness of 95 mg. Thedyeing was more level and the dyed strength greater than obtainablewithout the ethyl cellulose emulsion. The fabric also showed superiordye fastness and retained its stiffness after laundering.

Example V Five hundred parts by weight of 'the concentrated ethylcellulose emulsion used in Example III were diluted with 1,000 parts byweight of water containing 3.75 parts by weight of Pontamine sky blueFF. The mixture contained 0.25% of the dye. The ydilllted emulsion wasthen used to simultaneously dye and impregnate 2.85 yard sheeting by theprocedure described in I. The dyed fabric obtained was full and still,having a stiffness of 88.3 mg.. The dyed color was stronger thanobtainable without use ofthe ethyl cellulose emulsion and showed greaterretention of color after washing. Example VII The following solutionswere prepared:

Five hundred parts by weight of the concentrated emulsion were thendiluted with 1,000 parts by weight of water containing 3.7.5 parts byweight of Pontamine fast red BBL. The dyestuff was incorporated in thewater phase by the procedure described in Example I. The dilutedemulsion containing the 'dyestufi was used to simultaneously impregnateand dye 2.85 yard sheeting using the procedure described in Example I. Astill and full-bodied, dyed fabric was obtained having a stiffness of 69mg., as measured on the Gurley Stiffness tester. The fabric showed animproved dyed shade over that obtainable without the ethyl celluloseemulsion. The fabric was dyed fast and retained its stiffness after;laundering. 1 Example VIII The following solutions were prepared:

Parts by weight (a) Ethyl cellulose 32 Hydrogenated napthalene polymer,

M. P. C 10 Triphenyl phosphate 16 Xylol 106 Hi flash naphtha 20 Butanol16 Total 200 (b) Potassium oleaten' -I' 1.5 Water 98.5 Total lo (rSolutions (a) and (b) were emulsified as in Example I.

Five hundred parts by weight of the concentrated emulsion were dilutedwith 1,000 parts by weight of water containing 3.75 parts by weight ofPontamine fast red BBL. The diluted emulsion containing 0.25% by weightof the dyestuif was then used to simultaneously impregnate and dye 2.85yard sheeting by the procedure describedin Example I. The dyed fabricobtained was full-bodied and stiff, having a stiffness of 56 m. a

The dyed shade and the stiffness of the fabric were retained afterwashing.

The method of simultaneously dyeing and finishing textile fabrics inaccordance with this invention enables one to obtain in a singleoperation a dyed and finished fabric. By simultaneously dyeing andfinishing a textile fabric with an aqueous emulsion of awater-immiscible solution of water-insoluble ethyl cellulose containingin the water phase a direct water-soluble dyestufi, a dyed and finishedtextile fabric of improved properties is obtained, in accordance withthis invention. The strength of the dyed shade and the levelness of thedyed fabric are superior to that obtainable by dyeing the fabric with awater solution of the dye, as in common practice.

It will be understood that the details and examples hereinbefore setforth are illustrative only and that the invention as herein broadlydescribed and claimed is in no way limited thereby.

This application forms a continuation-in-part f of my application SerialNo. 128,039 filed February 26, 1937 entitled Textile Fabrics and Methodsof Preparation Thereof.

What I claim and desire to protect by Letters Patent is:

1. Process of simultaneously finishing and dyeing a textile fabric-toprovide in one operation a permanently finished, dyed fabric of opentexture which comprises immersing a textile fabric in an aqueousemulsion of a Water-immiscible solution of water-insoluble ethylcellulose, said aqueous emulsion containing in the aqueous, continuousphase a water-soluble direct dye, removing the excess emulsion from thefabric so as to leave in the fabric, on drying, an amount of solids.insufficient to fill the interstices between the threads or to form acontinuous coating over the surface of the fabric, drying the fabric,and ironing the fabric.

2. Process of simultaneously finishing and dyeing a textile fabric toprovide in one operation a permanently finished, dyed fabric of opentexture which comprises immersing a textile fabric in an aqueousemulsion of a water-immiscible solution of water-insoluble ethylcellulose and a plasticizer therefor which is resistant to alkalinesolutions, said aqueous emulsion containing in the aqueous, continuousphase a water-soluble direct dye, removing the excess emulsion from thefabric so as to leave in the fabric, on drying, an amount of solidsinsufficient to fill the inter stices between the threads or to form acontinuous coating over the surface of the fabric, drying the fabric,and ironing the fabric.

3. Process of simultaneously finishing and dyeing a textile fabric toprovide in one operation a permanently finished, dyed fabric of opentexture which comprises immersing a textile fabric in an aqueousemulsion of a water-immiscible solution of water-insoluble ethylcellulose and a plasticizer therefor which is resistant to alkalinesolutions and a thermoplastic alkali-resistant said aqueous emulsioncontaining in the aqueous,

continuous phase a water-soluble direct dye, removing the excessemulsion from the fabric so as to leave in the fabric, on drying, anamount of solids insufficient to fill the interstices between thethreads or to form a continuous coating over the surface of the fabric,drying the fabric, and ironing the fabric.

4. Process of simultaneously finishing and dyeing a textile fabric toprovide in one operation a permanently finished, dyed fabric of opentexture which comprises immersing a textile fabric in an aqueousemulsion of a water-immiscible solution of water-insoluble ethylcellulose and a plasticizer therefor which is resistant to alkalinesolutions and a thermoplastic alkali-resistant polymerized hydrocarbonresin compatible withethyl cellulose, said aqueous emulsion containingin the aqueous, continuous phase a watersoluble direct dye, removing theexcess emulsion from the fabric so as to leave in the fabric, on drying,an amount of solids insufficient to fill the interstices between thethreads or to form a continuous coating over the surface of the fabric,drying the fabric, and ironing the fabric.

5. Process of simultaneously finishing and dyeing a textile fabric toprovide in one operation a permanently finished, dyed fabric of opentexture which comprises immersing a textile fabric in an aqueousemulsion of a water-immiscible solution of water-insoluble ethylcellulose and a plasticizer therefor which is resistant to alkalinesolutions and a thermoplastic alkali-resistant rosin-modified alkydresin compatible with ethyl cellulose, said aqueous emulsion containingin the aqueous, continuous phase a water-soluble direct.

; ture which comprises immersing a textile fabric in an aqueous emulsionof a water-immiscible solution of water-insoluble ethyl cellulose and aplasticizer therefor which is resistant to alkaline solutions and apolyhydric alcohol ester of hydrogenated rosin, said aqueous emulsioncontaining in the aqueous, continuous phase a. watersoluble direct dye,removing the excess emulsion from the fabric so as to leave in thefabric, on drying, an amount of solids insufficient to fill theinterstices between the threads or to form a continuous coating over thesurface of the fabric, drying the fabric, and ironing the fabric.

7. Process of simultaneously finishing and dyeing a textile fabric toprovide in one operation a permanently finished, dyed fabric of opentexture which comprises immersing a textile fabric in an aqueousemulsion of a water-immiscible solution of water-insoluble ethylcellulose, said aqueous emulsion containing in the aqueous, continuousphase a water-soluble direct dye, removing the excess emulsion from thefabric so as to leave in the fabric, on drying, an amount of solidsinsufficient to fill the interstices between the threads or to form acontinuous coating over the surface of the fabric, drying the fabric,and ironing the fabric at a temperature within the range of about 180 toabout 400 F.

WILLIAM W. TROWELL.

